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 Post subject: Quantitative water test, I'm guessing this is the next step
PostPosted: Fri Jul 22, 2005 1:19 pm 
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Location: some where in the US midwest
Quantitative water test procedure for vegetable oil or biodiesel.

If you make biodiesel using vegetable oil that is contaminated with water, you can have problems. And the more water in the oil, the more problems you’ll have. Glop problems, washing/emulsion problems, reduced yield and so on. So here’s a way to actually test your oil to find out if it is contaminated with water or not, and if so, how much water. Please note that you can’t just look at the oil and know if it’s wet or not. It’s easy, so jump right on in. The short version is: weigh, heat to dry, weigh again, do math.

You need an accurate scale that can precisely measure weight with a resolution of 0.1 grams (a tenth of a gram) or better. Ebay has lots of vendors that can supply a manual triple beam balance that works beautifully. There are digital versions as well. The scale should have an upper capacity of about 500g or more to do this test well. You could fake it with a top capacity of 100g, but you have to use a much smaller sample and you lose some precision.

1. Find a container to put an oil sample in. Gladware works nicely (semi-disposable “Tupperware” and available at any supermarket or Wal-Mart). It’s about the right size, cheap, lightweight, re-usable, see-through and heat resistant at the temperatures we’re working with.

2. Weigh the empty container to the nearest tenth of a gram and record that somewhere.

3. Take a 300 to 400 mL sample of oil. The sample should be representative of all the oil you are going to react. So typically, I dump all my oil into my processor tank and stir it for ten or fifteen minutes. Then I take the sample.

4. Weigh the sample. Record this number. Subtracting the weight of the container gives us the actual weight of the oil. Record oil weight. I designate this as “wet weight”.

5. Heat the sample in a microwave until the oil reaches a temperature of 250F(~120C). Test the temperature of the oil periodically OUT OF THE MICROWAVE. Keep it at this temperature until all boiling stops. You should heat for a minute or two and then test the temperature. Then heat again, and check temp.

Harbor Freight sells a nice probe thermometer with a 6” metal probe with a round thermometer head at the end. A candy thermometer would work as well. Check your thermometer for accuracy in boiling water and confirm a reading around 212F (100C). Some are a mile off. During the heating phase, you will get a qualitative indication for the presence of water. If your sample starts to spit and boil around 212F (100C) you know there is some water. We’ll get quantitative data in a few minutes.

6. Allow the sample to cool off for ten minutes or so. This allows any residual emulsified water to evaporate, plus it’s safer.

7. Weigh the sample again, record that number. Subtract container weight. This is your “dry weight” of the oil. If you’re a purist from chem. lab, you would do the whole heat/weigh thing again and again until the weight stops going down to be sure the water is all gone. I make the assumption that if the sample is 250F(~120C) and there’s no boiling, the water is gone.

8. You can see where this is going. Take wet weight and subtract dry weight. The difference is the weight of the water that was in your sample. Now divide water weight by the original “wet oil weight” and this will give the decimal fraction water content of the sample. Multiply by 100 to get percent.

Here’s an example:

Container wt: 26.2g
Total wet wt: 335.6g
Wet oil wt: 335.6g - 26.2g = 309.4g
Total dry wt: 321.6g
Dry oil wt: 321.6g – 26.2g = 297.4g
Water wt: 309.4g – 297.4 = 12.0g water
Water content: 12.0g / 309.4g = 0.03878
% water by wt: 0.03878 x 100 ~ 3.9% water by weight

If I’m careful, and without heroics, I can measure the presence of 0.2 grams of water in a 500 gram oil sample. That would be:

0.2g/500g = 0.0004 water, or 0.04% water.

So even if you’re sloppy, and only measure gram amounts, you can still learn a lot about water content with a scale and a microwave. As an example, my microwave is 1,100 watts and I do the test on high for 3-6 minutes, depending on how cold and how wet the oil is. I typically do one or two minutes per session and then check temperature. It has crossed my mind you could use the defrost function for really wet oil to minimize popping issues if needed. If it pops a lot, you could be losing oil and it will make your results look wetter than it reallly is. It would take longer of course, but it's basically an unsupervised process. Nuke for ten minutes on defrost and check temp, etc.

Summary:

Weigh
Heat
Weigh again
Do math stuff

Good luck and have fun!
Troy

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 Post subject:
PostPosted: Fri Jul 22, 2005 3:11 pm 
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any chance you could take some pictures to go with this? I can also send you a cheap digital camera, or I can scan in old-fashioned paper photos of yours, if that'll help.

Mark


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 Post subject:
PostPosted: Fri Jul 22, 2005 10:17 pm 
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Joined: Tue Dec 21, 2004 6:49 pm
Posts: 173
Location: Utah
I'll watch for some photo's in the next few days & then I'll throw this up on the site.
-Graydon


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 Post subject:
PostPosted: Sat Jul 23, 2005 11:53 am 
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Joined: Mon Jul 11, 2005 11:16 am
Posts: 22
Location: some where in the US midwest
I have a digital camera. How does one make the image available on this site?

Alternatively, I could incorporate the photos into the article (a Word document originally) and post that. Can I just copy the article with photos and post them in that fashion?

Alternate #2, I could email some photos to somebody that's web-handy and they could put them in as they see fit.

I was at something of a loss as to what photos...

-triple beam balance?
-gladware?
-probe thermometer?

Finest regards,

troy

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 Post subject:
PostPosted: Sat Jul 23, 2005 8:31 pm 
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when you post a 'reply' to this post, you'll see a box at the bottom for attaching images or other files. From therre on , it's just like attaching files to an email- click 'browse' and it'll let you look through your hard drive looking for the appropriate file.
I found that it's a pain to remove images from Word in order to make them available for html, so please just attach a .jpg separately rather than in word format...

mark


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 Post subject:
PostPosted: Mon Jul 25, 2005 3:11 pm 
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Joined: Tue Dec 21, 2004 6:49 pm
Posts: 173
Location: Utah
For which pictures to use, think of it like a visual tutorial guide.
It's good to get pictures of every step you'd do to do the test.

A good example is the Emulsion Article and the Titrating Oil article.
Good pictures every step of the way.

Hope that helps.
-Graydon


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 Post subject:
PostPosted: Tue Jul 26, 2005 5:00 am 
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and if you want to mess with people's heads, you can just copy some photos of a glowing microwave out of the 'grape plasma' web page:
http://c3po.barnesos.net/homepage/lpl/grapeplasma/

Mark


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 Post subject:
PostPosted: Wed Jul 27, 2005 1:04 pm 
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Location: some where in the US midwest
Gimme a week to produce some photos.

finest regards,

troy

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 Post subject:
PostPosted: Fri Jul 29, 2005 12:46 pm 
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Location: S.E. England
Nice one with your article troy

and I know it's useful to you guys in the USA but I'm wondering about the references to stores for buying supplies, they don't mean a lot to anyone reading this from outside the USA, and we are trying to reach a global market?

Chug

it's right in the middle of my silly season with straw bale building and I am not finding much time to keep up with biofuel stuff.


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 Post subject: OK, here's the only two meaningful photos
PostPosted: Mon Aug 01, 2005 9:43 pm 
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Location: some where in the US midwest
Since I have a new laptop, new photo software, etc, I am not totally confident that the photos will be of the appropriate size and quality. If now, we'll fiddle around some more.

Finest regards,

troy


Attachments:
thermometer resize 1.jpg
thermometer resize 1.jpg [ 132.87 KiB | Viewed 6812 times ]
resize 750 microwave.jpg
resize 750 microwave.jpg [ 181.78 KiB | Viewed 6807 times ]

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 Post subject: photo size
PostPosted: Mon Aug 01, 2005 9:49 pm 
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Location: some where in the US midwest
OK then,

My initial reaction to the posted photos is that they are bigger than necessary. If there is any concurence, I'll repost smaller versions. Graydon (or whoever would like to integrate the photos and the text), could you add a caption to the thermometer photo noting that the dial has lapped itself so to speak, and is indicating approx 260F.

Finest regards,

troy

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 Post subject:
PostPosted: Mon Aug 01, 2005 9:57 pm 
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Joined: Mon Jul 11, 2005 11:16 am
Posts: 22
Location: some where in the US midwest
Chug wrote:
Nice one with your article troy

and I know it's useful to you guys in the USA but I'm wondering about the references to stores for buying supplies, they don't mean a lot to anyone reading this from outside the USA, and we are trying to reach a global market?


Chug, that is a point well taken. But I am unsure what to do about it. I could delete the reference to the U.S. source, which doesn't help anybody. Or I could make some appologies in advance since I have no way of adding sources for the folks not in North America, but that is just a feel good measure that doesn't help out the rest of you either.

Well fiddle faddle...

Open to suggestions...

Finest regards,

troy

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 Post subject:
PostPosted: Tue Aug 02, 2005 11:44 am 
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as for photos, I like to have us 'host' large photos but re-size them in the html so they appear smaller in your browser. The point is that someone could click on the photo and see it larger if desired, or grab it for use in a presentation, etc.

Mark


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 Post subject: Are we ready then?
PostPosted: Wed Aug 03, 2005 8:40 am 
So I may assume, by the dissappearance of the photos that someone has taken care of the size issue?

And that we are ready for publication?

If so, wooooo hooooooooo!

Having way to much fun for a grown man.

troy


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 Post subject:
PostPosted: Wed Aug 03, 2005 2:17 pm 
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if i understand correctly you just didnt' see them because you weren't signed in. (you just posted as guest- oops, gotta turn off guest posting)

Mark


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